顶空气相色谱法测定双氯芬酸钠缓释胶囊中丙酮和乙醇残留量

Determination of Residual Amount of Acetone and Ethanol in Diclofenac Sodium Sustained-Release Capsules by HS-GC

目的建立测定双氯芬酸钠缓释胶囊中丙酮和乙醇残留量的顶空气相色谱法。方法色谱柱为Agilent HP-FFAP毛细管气相色谱柱（30 m×0.320 m,0.25μm）,柱温为40℃,进样口温度为180℃,FID检测器温度为240℃,顶空瓶平衡温度为85℃,平衡时间为30 min,进样量为1 m L,载气为氮气,流速为2.0 m L/min。结果丙酮、乙醇质量浓度分别在0.102 10~2.042 00 g/L（r=0.999 9）和0.102 51~2.050 20 g/L（r=1.000 0）范围内与峰面积呈良好线性关系（n=6）,平均回收率分别为99.00%（RSD=0.98%,n=6）和101.54%（RSD=0.48%,n=6）。结论该方法简单、准确、重复性好,可用于双氯芬酸钠缓释胶囊中丙酮、乙醇残留量的测定。

Objective To establish a headspace gas chromatography（ HS- GC） method for determining the residual amountof acetone and ethanol in Diclofenac Sodium Sustained- Release Capsules. Methods The Agilent HP- FFAP capillary column（ 30 m × 0. 320 m,0. 25 μm）was used as the chromatographic column. The column temperature was 40 ℃. The injection port temperature was 180 ℃. The FID detector temperature was 240 ℃. The equilibrium temperature of the headspace gas bottle was 85 ℃. The equilibrium time was 30 minutes. The injection volume was 1 m L. The carrier gas was nitrogen. The flow rate was 2. 0 m L / min. Results The mass concentrations in the range of0. 102 10- 2. 042 00 g / L for acetone（ r = 0. 999 9） and in the range of 0. 102 51- 2. 050 20 g / L for ethanol（ r = 1. 000 0） showed good linear relation with the peak area. The average recovery rates of acetone and ethanol were 99. 00%（ RSD = 0. 98%,n = 6） and101. 54%（ RSD = 0. 48%,n = 6）. Conclusion The established method is simple,accurate and repeatable,which can be applied to determine the residual amount of acetone and ethanol in Diclofenac Sodium Sustained- Release Capsules.